JP5456541B2 - Ultra-thin beryllium foil and manufacturing method thereof - Google Patents
Ultra-thin beryllium foil and manufacturing method thereof Download PDFInfo
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- JP5456541B2 JP5456541B2 JP2010082065A JP2010082065A JP5456541B2 JP 5456541 B2 JP5456541 B2 JP 5456541B2 JP 2010082065 A JP2010082065 A JP 2010082065A JP 2010082065 A JP2010082065 A JP 2010082065A JP 5456541 B2 JP5456541 B2 JP 5456541B2
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- 229910052790 beryllium Inorganic materials 0.000 title claims description 109
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 title claims description 109
- 239000011888 foil Substances 0.000 title claims description 96
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 238000005096 rolling process Methods 0.000 claims description 64
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 34
- 230000007547 defect Effects 0.000 claims description 34
- 229910052582 BN Inorganic materials 0.000 claims description 28
- 229910001220 stainless steel Inorganic materials 0.000 claims description 22
- 239000010935 stainless steel Substances 0.000 claims description 21
- 238000005098 hot rolling Methods 0.000 claims description 13
- 239000000314 lubricant Substances 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 230000005540 biological transmission Effects 0.000 claims description 5
- 238000000034 method Methods 0.000 description 30
- 239000000463 material Substances 0.000 description 13
- 238000010894 electron beam technology Methods 0.000 description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- 206010070834 Sensitisation Diseases 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000008313 sensitization Effects 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910001105 martensitic stainless steel Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
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Description
本発明は、超薄膜ベリリウム箔及びその製造方法に関する。 The present invention relates to an ultra-thin beryllium foil and a method for manufacturing the same.
ベリリウム箔は、Ｘ線や電子線の透過率が高いことから、Ｘ線発生装置のＸ線用窓材や電子線発生装置の電子線用窓材として用いられている（例えば特許文献１参照）。こうしたベリリウム箔は、厚さが薄いほど透過率が高くエネルギーロスも小さいことから好ましい。 Beryllium foil is used as an X-ray window material for an X-ray generator and an electron beam window material for an electron beam generator because of its high X-ray and electron beam transmittance (see, for example, Patent Document 1). . Such beryllium foil is preferable because the thinner the thickness, the higher the transmittance and the smaller the energy loss.
しかしながら、ベリリウムは、一般の金属材料と異なり、延性が小さく、室温で塑性加工することは困難である。具体的には、酸化防止のためにステンレス鋼板などのシースで原料のベリリウム板を挟み込んだ状態で加熱し、圧延機に挿入することが考えられるが、その場合には、ベリリウム箔がステンレス鋼板と密着し、剥離する際に、ベリリウムが破れたり、加熱により鋭敏化したステンレスが脱落し、ベリリウムに押し込まれ貫通したりすることで、ベリリウムに穴が生じ、それが窓材として必要な真空気密性を阻害する欠陥となる。この点を改善しようとして、ベリリウム板とシースとの間に密着防止のための固体潤滑剤を塗布すると、最終的に固体潤滑剤がベリリウム箔の表面に残ってＸ線や電子線の透過率に悪影響を及ぼすことがあった。なお、例えば、特許文献１の特許請求の範囲には厚さが１０〜１００μｍの範囲のベリリウム箔を用いた真空容器が記載されているものの、実施例で用いられているベリリウム箔は厚さが６０μｍのものと８９μｍのものにすぎない。 However, unlike general metal materials, beryllium has small ductility and is difficult to be plastically processed at room temperature. Specifically, for prevention of oxidation, it is conceivable that the raw material beryllium plate is sandwiched between sheaths such as a stainless steel plate and inserted into a rolling mill. When adhering and peeling, the beryllium breaks, or the stainless steel that has been sensitized by heating falls off, being pushed into the beryllium and penetrating into it, creating a hole in the beryllium, which is the vacuum tightness required as a window material It becomes a defect that inhibits. In order to improve this point, if a solid lubricant for preventing adhesion is applied between the beryllium plate and the sheath, the solid lubricant will eventually remain on the surface of the beryllium foil, resulting in an increase in the transmittance of X-rays and electron beams. There was an adverse effect. For example, although the vacuum vessel using the beryllium foil having a thickness in the range of 10 to 100 μm is described in the claims of Patent Document 1, the beryllium foil used in the examples has a thickness of They are only 60 μm and 89 μm.
本発明はこのような課題を解決するためになされたものであり、厚さ１０μｍ程度でありながら欠陥密度が小さくかつ、リーク量が小さく真空気密性に優れた大面積のベリリウム箔を提供することを主目的とする。 The present invention has been made to solve such a problem, and provides a large-area beryllium foil having a small defect density, a small leak amount, and an excellent vacuum tightness while having a thickness of about 10 μm. The main purpose.
本発明者らは、厚肉のベリリウム板を熱間圧延加工を繰り返すことにより薄肉化して厚さ１０μｍ程度のベリリウム箔を製造する方法を鋭意検討した。その結果、シースとベリリウム板との間に固体潤滑剤として窒化ボロン（ＢＮ）を塗布すると、圧延加工時にシースとベリリウム箔とが密着するのを防止すると共に欠陥密度を有効に抑制できることを見いだした。また、熱間圧延加工を繰り返し行うにあたり、シースの延性が低下する前に新たなシースでベリリウム板を挟み直す必要があるが、その際にベリリウム板をある厚さまで薄肉化したら、それ以降はＢＮを用いることなく目的とする１０μｍ程度の厚さに仕上げることが最終品にＢＮを残留させないのに有効であると共に、ＢＮを使用していないにもかかわらず、シースとベリリウム板との密着がほとんど起こらなくなることを見いだした。こうした知見をもとに、本発明者らは本発明を完成するに至った。 The inventors diligently studied a method for manufacturing a beryllium foil having a thickness of about 10 μm by thinning a thick beryllium plate by repeating hot rolling. As a result, when boron nitride (BN) was applied as a solid lubricant between the sheath and the beryllium plate, it was found that the sheath and beryllium foil were prevented from sticking during rolling and the defect density could be effectively suppressed. . In addition, when the hot rolling process is repeated, it is necessary to sandwich the beryllium plate with a new sheath before the ductility of the sheath is lowered. If the beryllium plate is thinned to a certain thickness at that time, then BN Finishing to the target thickness of about 10 μm without using BN is effective in preventing BN from remaining in the final product, and in spite of the absence of BN, there is almost no adhesion between the sheath and the beryllium plate. I found that it didn't happen. Based on these findings, the present inventors have completed the present invention.
本発明の超薄膜ベリリウム箔の製造方法は、ベリリウム箔とステンレス鋼からなる一対のシースとの間に固体潤滑剤である窒化ホウ素（ＢＮ）を塗布してなる積層体を作製し、該積層体の熱間圧延加工を繰り返し行う、第１の圧延工程と、ベリリウム箔とステンレス鋼からなる一対のシースとの間にＢＮを塗布することなく積層体を作製し、該積層体の熱間圧延加工を繰り返し行う、第２の圧延工程とを実行するにあたり、ベリリウム箔の厚さが１５〜６０μｍの間で定められた所定のしきい値以下になっていない場合には、前記第１の圧延工程を繰り返し実行し、その後、ベリリウム箔の厚さが前記しきい値以下になった場合には、前記第２の圧延工程をベリリウム箔の厚さが５〜２０μｍの間で前記しきい値より小さい値に定められた目標厚さになるまで繰り返し実行するものである。 The manufacturing method of the ultra-thin beryllium foil of the present invention produces a laminated body obtained by applying boron nitride (BN), which is a solid lubricant, between a beryllium foil and a pair of sheaths made of stainless steel. A laminate is produced without applying BN between the first rolling step and the pair of sheaths made of beryllium foil and stainless steel, and the hot rolling of the laminate is repeated. When the thickness of the beryllium foil is not less than or equal to a predetermined threshold value determined between 15 and 60 μm in performing the second rolling step, the first rolling step is repeated. Is repeated, and when the beryllium foil thickness is less than or equal to the threshold value, the second rolling step is performed with the beryllium foil thickness being between 5 and 20 μm and less than the threshold value. Target set by value This is repeated until the thickness is reached.
本発明の超薄膜ベリリウム箔は、厚さ５〜２０μｍ、面積１０００ｍｍ2以上、光透過により測定される欠陥個数がゼロのものでかつ、リーク量が１×１０−10Ｐａ・ｍ／ｓｅｃ以下である。 The ultra-thin beryllium foil of the present invention has a thickness of 5 to 20 μm, an area of 1000 mm 2 or more, the number of defects measured by light transmission is zero, and the leak amount is 1 × 10 −10 Pa · m / sec or less. is there.
本発明の超薄膜ベリリウム箔の製造方法では、ベリリウム箔の厚さが所定のしきい値以下になっていない場合には、ＢＮの塗布を伴う第１の圧延工程を繰り返し実行する。この第１の圧延工程では、ベリリウム箔とこれを挟み込む一対のシースとの間に固体潤滑剤としてのＢＮが介在しているため、圧延加工後にベリリウム箔とシースとが密着して剥がすのが困難になるという事態を招くことはない。一方、ベリリウム箔の厚さが目標厚さになるまで第１の圧延工程を繰り返すと、最終的に得られるベリリウム箔にＢＮが残存してＸ線や電子線の透過性能に悪影響を及ぼすおそれがあるが、本発明では、ベリリウム箔の厚さが所定のしきい値以下になったあとはＢＮの塗布を行わない第２の圧延工程を実行するため、最終的に得られるベリリウム箔にＢＮが残留しない。また、第２の圧延工程では、ＢＮを使用していないにもかかわらずシースとベリリウム板との密着がほとんど起こらないし、欠陥の発生も有効に抑制される。その結果、本発明の製造方法によれば、厚さ１０μｍ程度でありながら欠陥密度が小さくかつ、リーク量が小さく真空気密性に優れ、圧延加工時の固体潤滑剤が残留しないベリリウム箔が得られる。 In the manufacturing method of the ultra-thin beryllium foil of the present invention, when the thickness of the beryllium foil is not less than or equal to a predetermined threshold value, the first rolling process with BN coating is repeatedly executed. In this first rolling step, BN as a solid lubricant is interposed between the beryllium foil and a pair of sheaths sandwiching the beryllium foil, so that it is difficult for the beryllium foil and the sheath to come into close contact with each other after the rolling process. The situation of becoming will not be invited. On the other hand, if the first rolling process is repeated until the beryllium foil thickness reaches the target thickness, BN may remain in the finally obtained beryllium foil, which may adversely affect the transmission performance of X-rays and electron beams. However, in the present invention, since the second rolling process in which BN is not applied is performed after the thickness of the beryllium foil becomes a predetermined threshold value or less, BN is added to the finally obtained beryllium foil. Does not remain. In addition, in the second rolling process, despite the fact that BN is not used, the sheath and the beryllium plate hardly adhere to each other, and the occurrence of defects is effectively suppressed. As a result, according to the production method of the present invention, a beryllium foil having a thickness of about 10 μm, a small defect density, a small amount of leakage, excellent vacuum tightness, and no solid lubricant remaining during rolling can be obtained. .
なお、第１の圧延工程から第２の圧延工程に切り替える際、第１の圧延工程後のベリリウム箔にはＢＮが残留しているが、最終的にそのＢＮがベリリウム箔に残留しないのは、おそらくその後の第２の圧延工程においてベリリウム箔上のＢＮがシース側に付着して除去されるからと推察している。また、第２の圧延工程では、ベリリウム箔とシースとの間にＢＮを塗布していないにもかかわらず、ベリリウム箔とシースとが密着してしまうことがないが、その理由は第１の圧延でベリリウムの表面に残留しているＢＮが第２の圧延中に除去されつつ、密着防止の効果も持続していることによるものと推察する。 Note that when switching from the first rolling process to the second rolling process, BN remains in the beryllium foil after the first rolling process, but the BN does not remain in the beryllium foil in the end. Presumably, BN on the beryllium foil adheres to the sheath side and is removed in the subsequent second rolling step. In the second rolling step, the beryllium foil and the sheath do not adhere to each other even though BN is not applied between the beryllium foil and the sheath. It is assumed that BN remaining on the surface of beryllium is removed during the second rolling and that the effect of preventing adhesion is maintained.
本発明の超薄膜ベリリウム箔によれば、厚さが非常に薄いため、Ｘ線や電子線が透過しやすくエネルギーロスが少ない。しかも、超薄膜であるにもかかわらず気体がほとんどリークしない。また、ベリリウム箔としては異例の１０００ｍｍ2以上という大面積であるため、例えばＸ線用窓材や電子線用窓材を大型化することができる。 According to the ultra-thin beryllium foil of the present invention, since the thickness is very thin, X-rays and electron beams are easily transmitted and there is little energy loss. In addition, the gas hardly leaks despite the ultrathin film. Moreover, since it is an unusual large area of 1000 mm < 2 > or more as beryllium foil, the window material for X-rays and the window material for electron beams can be enlarged, for example.
本発明の超薄膜ベリリウム箔の製造方法において、第１の圧延工程では、ベリリウム箔とステンレス鋼からなる一対のシースとの間に固体潤滑剤であるＢＮを塗布してなる積層体を作製し、該積層体の熱間圧延加工を繰り返し行う。また、 第２の圧延工程では、ベリリウム箔とステンレス鋼からなる一対のシースとの間にＢＮを塗布することなく積層体を作製し、該積層体の熱間圧延加工を繰り返し行う。 In the manufacturing method of the ultra-thin beryllium foil of the present invention, in the first rolling step, a laminate formed by applying BN, which is a solid lubricant, between a pair of sheaths made of beryllium foil and stainless steel, The laminate is repeatedly subjected to hot rolling. In the second rolling step, a laminate is produced without applying BN between the beryllium foil and a pair of sheaths made of stainless steel, and the hot rolling of the laminate is repeated.
ここで、ベリリウム箔としては、特に限定されないが、純度９８％以上のものが好ましく、特に純度が９９％以上のものがより好ましい。シースとしては、軟鋼やステンレス鋼製が望ましいが、ステンレス鋼については、オーステナイト系ステンレス鋼製（例えばＳＵＳ３０４，ＳＵＳ３１６など）やマルテンサイト系ステンレス鋼製（例えばＳＵＳ４０３など）、フェライト系ステンレス鋼製（例えばＳＵＳ４０５など）が挙げられる。このうちオーステナイト系ステンレス鋼製のものがより好ましい。固体潤滑剤としては、ＢＮを使用する。二硫化モリブデンなど他の固体潤滑剤では、圧延時の温度に対し十分な耐熱性が無いため、ベリリウム箔とシースとの密着を有効に防止することができないからである。ＢＮは、スプレーで塗布してもよいし、ローラーやハケで塗布してもよい。ベリリウム箔とステンレス鋼からなる一対のシースとの間に固体潤滑剤であるＢＮを塗布してなる積層体は、ベリリウム箔を挟み込んだ一対のシース同士を溶接やロウ付け等で一体化した上で、熱間圧延加工するのが好ましい。ステンレス鋼からなるシースは、熱間圧延加工を繰り返すにつれて徐々に硬くなり延性が低下する。このため、熱間圧延加工の加工率は、延性が維持される範囲で適宜設定するのが好ましい。なお、延性が維持されるとは、圧延の前後でシースの延びが確認できることをいう。熱間圧延加工では、圧延温度を３００〜１０００℃の間で設定するのが好ましく、５００〜７００℃の間で設定するのがより好ましい。また、圧延機としては、通常市販されているもの、例えば２段圧延機を利用すればよい。 Here, the beryllium foil is not particularly limited, but preferably has a purity of 98% or more, and more preferably has a purity of 99% or more. The sheath is preferably made of mild steel or stainless steel, but the stainless steel is made of austenitic stainless steel (eg SUS304, SUS316 etc.), martensitic stainless steel (eg SUS403 etc.), ferritic stainless steel (eg SUS405 etc.). Of these, those made of austenitic stainless steel are more preferred. BN is used as the solid lubricant. This is because other solid lubricants such as molybdenum disulfide do not have sufficient heat resistance with respect to the temperature during rolling, and thus the adhesion between the beryllium foil and the sheath cannot be effectively prevented. BN may be applied by spraying, or may be applied by a roller or a brush. The laminated body formed by applying BN, which is a solid lubricant, between a beryllium foil and a pair of stainless steel sheaths is obtained by integrating a pair of sheaths sandwiching the beryllium foil by welding or brazing. It is preferable to perform hot rolling. The sheath made of stainless steel is gradually hardened and the ductility is lowered as hot rolling is repeated. For this reason, it is preferable to set the processing rate of the hot rolling process appropriately within a range in which ductility is maintained. Note that maintaining ductility means that the extension of the sheath can be confirmed before and after rolling. In hot rolling, the rolling temperature is preferably set between 300 and 1000 ° C, more preferably between 500 and 700 ° C. Moreover, what is necessary is just to utilize what is marketed normally, for example, a two-high mill, as a rolling mill.
本発明の超薄膜ベリリウム箔の製造方法において、ベリリウム箔の厚さが１５〜６０μｍの間で定められた所定のしきい値以下になっていない場合には、第１の圧延工程を繰り返し実行し、その後、ベリリウム箔の厚さがしきい値以下になった場合には、第２の圧延工程をベリリウム箔の厚さが５〜２０μｍの間でしきい値より小さい値に定められた目標厚さになるまで繰り返し実行する。 In the manufacturing method of the ultra-thin beryllium foil of the present invention, when the thickness of the beryllium foil is not less than or equal to a predetermined threshold value defined between 15 to 60 μm, the first rolling step is repeatedly executed. Then, when the thickness of the beryllium foil falls below the threshold value, the second rolling process is performed to a target thickness that is set to a value smaller than the threshold value when the thickness of the beryllium foil is between 5 and 20 μm. Repeat until
ここで、しきい値は、ベリリウム箔の厚さが１５〜６０μｍの間で定められている。しきい値が１５μｍ未満の場合には、ＢＮの塗布が難しいため好ましくない。また、しきい値が６０μｍを超える場合には、第２の圧延工程で、ＢＮが完全に無くなり、ステンレス鋼と密着する可能性が高いため好ましくない。また、目標厚さは、５〜２０μｍの間で定められている。目標厚さが５μｍ未満の場合には、厚さが薄すぎて熱間圧延加工を実行する際に破損しやすいため好ましくない。また、目標厚さが２０μｍを超える場合には、第２の圧延工程だけでも良好なベリリウム箔を得ることが出来るため、本発明の方法を適用する意義が低い。このように極めて薄いベリリウム箔は、他の方法では作製するのが極めて困難であるため、本発明の方法を適用する意義が高い。 Here, the threshold value is determined when the thickness of the beryllium foil is between 15 and 60 μm. When the threshold value is less than 15 μm, it is difficult to apply BN, which is not preferable. In addition, when the threshold value exceeds 60 μm, BN is completely eliminated in the second rolling step, which is not preferable because there is a high possibility of being in close contact with stainless steel. The target thickness is determined between 5 and 20 μm. When the target thickness is less than 5 μm, it is not preferable because the thickness is too thin and is easily damaged when hot rolling is performed. In addition, when the target thickness exceeds 20 μm, a good beryllium foil can be obtained only by the second rolling step, so that the significance of applying the method of the present invention is low. Such an extremely thin beryllium foil is extremely difficult to produce by other methods, and therefore, the significance of applying the method of the present invention is high.
本発明の超薄膜ベリリウム箔の製造方法において、シースは、カーボン含有率０．０３重量％以下のステンレス鋼からなることが好ましい。カーボン含有率が０．０３重量％を超えるステンレス鋼からなるシースを用いて熱間圧延加工を行うと、ステンレス鋼が鋭敏化により脆弱になりやすく、シースから結晶粒が脱落してベリリウム箔に押し込まれ、穴を開けることがある。そのように結晶粒が脱落するのは、熱間加工時に結晶粒界にカーボンが集まって起こる鋭敏化が原因と考えられる。 In the method for producing an ultrathin beryllium foil of the present invention, the sheath is preferably made of stainless steel having a carbon content of 0.03% by weight or less. When hot rolling is performed using a sheath made of stainless steel having a carbon content of over 0.03% by weight, the stainless steel tends to become brittle due to sensitization, and crystal grains fall off from the sheath and are pushed into the beryllium foil. And may make holes. It is thought that the crystal grains fall off due to the sensitization caused by carbon gathering at the crystal grain boundaries during hot working.
本発明の超薄膜ベリリウム箔は、厚さ５〜２０μｍ、面積１０００ｍｍ2以上、光透過により測定される欠陥個数がゼロのものである。こうした超薄膜ベリリウム箔は、上述した超薄膜ベリリウム箔の製造方法で厚さ５〜２０μｍのベリリウム箔を作製したあと、欠陥個数がゼロで面積の大きなところを切り出すことにより得ることができる。欠陥個数は、超薄膜ベリリウム箔の裏面から光を照射したときに表側に光が透過した部位をカウントしたものである。この超薄膜ベリリウム箔は、空気の漏れ試験を行ったときに、リークレート値が１×１０-8Ｐａ・ｍ3／ｓｅｃ以下であることが好ましく、リークレート値が１×１０-10Ｐａ・ｍ3／ｓｅｃ以下であることがより好ましい。リークレートに対する要求値は、使用される用途において必要な真空度により、変わるが、リークレートが小さいほど、より高真空度を必要とする用途で使用することが可能である。 The ultra-thin beryllium foil of the present invention has a thickness of 5 to 20 μm, an area of 1000 mm 2 or more, and zero defects measured by light transmission. Such an ultra-thin beryllium foil can be obtained by producing a beryllium foil having a thickness of 5 to 20 μm by the above-described method for producing an ultra-thin beryllium foil and then cutting out a large area with zero defects. The number of defects is the number of sites where light is transmitted to the front side when light is irradiated from the back surface of the ultrathin beryllium foil. The ultra-thin beryllium foil preferably has a leak rate value of 1 × 10 −8 Pa · m 3 / sec or less when an air leak test is performed, and has a leak rate value of 1 × 10 −10 Pa · More preferably, it is m 3 / sec or less. The required value for the leak rate varies depending on the degree of vacuum required in the application to be used. However, the smaller the leak rate, the higher the degree of vacuum can be used.
［一般的手順］
Ａ：第１の圧延工程は、以下の手順により実施した。なお、手順Ａ１〜Ａ６の一連の操作をチャンネル（ｃｈ）と称する。
（手順Ａ１）加工対象品のベリリウム箔の両面にＢＮをスプレーした。なお、初回は、純度９９％以上のベリリウム箔（厚さ１ｍｍ）を用意し、研磨加工により厚さを７５０μｍとし、幅を１２０ｍｍにしたものを加工対象品とした。
（手順Ａ２）ＢＮをスプレーしたベリリウム箔をＳＵＳ３０４（カーボン含有率０．０７重量％）製の一対のシースで挟み込み、外周をＴＩＧ溶接して積層体とした。この積層体の平面図及び断面図を図１に示す。
（手順Ａ３）積層体を電気炉中で所定の圧延温度に加熱し保持した。
（手順Ａ４）上下ロールで板材を圧延する構造の２段圧延機を用意し、ロール間ギャップを設定した。
（手順Ａ５）加熱した積層体をロール間に通して圧延した。
（手順Ａ６）上述した手順Ａ３〜Ａ５を繰り返し、所定の厚みになるまで圧延した。具体的には、手順Ａ６で得られたベリリウム箔を新たに加工対象品として手順Ａ３以降を実施した。２段圧延機のロール間に通す回数をパス回数と呼ぶが、このパス回数が多くなるにつれてシースが硬くなるため、経験的にシースの延性が維持される範囲でパス回数を設定した。
[General procedure]
A: The 1st rolling process was implemented with the following procedures. A series of operations of procedures A1 to A6 is referred to as a channel (ch).
(Procedure A1) BN was sprayed on both surfaces of the beryllium foil of the product to be processed. In the first time, a beryllium foil (thickness 1 mm) having a purity of 99% or more was prepared, and a product with a thickness of 750 μm and a width of 120 mm was obtained by polishing.
(Procedure A2) A beryllium foil sprayed with BN was sandwiched between a pair of sheaths made of SUS304 (carbon content 0.07% by weight), and the outer periphery was TIG welded to obtain a laminate. A plan view and a cross-sectional view of this laminate are shown in FIG.
(Procedure A3) The laminate was heated and held at a predetermined rolling temperature in an electric furnace.
(Procedure A4) A two-high rolling mill having a structure for rolling plate material with upper and lower rolls was prepared, and a gap between rolls was set.
(Procedure A5) The heated laminate was rolled between rolls.
(Procedure A6) The above-described procedures A3 to A5 were repeated and rolled to a predetermined thickness. Specifically, the procedure A3 and subsequent steps were carried out using the beryllium foil obtained in the procedure A6 as a new product. The number of passes between the rolls of the two-high rolling mill is referred to as the number of passes. Since the sheath becomes harder as the number of passes increases, the number of passes is set empirically within a range in which the ductility of the sheath is maintained.
Ｂ：第２の圧延工程は、以下の手順により実施した。なお、手順Ｂ１〜Ｂ５の一連の操作もチャンネル（ｃｈ）と称する。
（手順Ｂ１）加工対象品のベリリウム箔の両面にＢＮをスプレーすることなく、ＳＵＳ３０４（カーボン含有率０．０７重量％）製の一対のシースで挟み込み、外周８箇所をＴＩＧ溶接して積層体とした。
（手順Ｂ２）積層体を電気炉中で所定の圧延温度に加熱し保持した。
（手順Ｂ３）上下ロールで板材を圧延する構造の２段圧延機を用意し、ロール間ギャップを設定した。
（手順Ｂ４）加熱した積層体をロール間に通して圧延した。
（手順Ｂ５）上述した手順Ｂ２〜Ｂ４を繰り返した。具体的には、手順Ｂ４で得られたベリリウム箔を新たに加工対象品として手順Ｂ２以降を実施した。また、パス回数が多くなるにつれてシースが硬くなるため、経験的にシースの延性が維持される範囲でパス回数を設定した。なお、手順Ｂ２〜Ｂ５は上述した手順Ａ３〜Ａ６と同じである。
B: The 2nd rolling process was implemented with the following procedures. Note that a series of operations in steps B1 to B5 is also referred to as a channel (ch).
(Procedure B1) Without spraying BN on both sides of the beryllium foil of the product to be processed, sandwiched by a pair of sheaths made of SUS304 (carbon content 0.07% by weight), and TIG welding the outer periphery 8 locations did.
(Procedure B2) The laminate was heated and held at a predetermined rolling temperature in an electric furnace.
(Procedure B3) A two-high rolling mill having a structure for rolling plate material with upper and lower rolls was prepared, and a gap between rolls was set.
(Procedure B4) The heated laminate was rolled between rolls.
(Procedure B5) The procedures B2 to B4 described above were repeated. Specifically, the procedure B2 and subsequent steps were carried out using the beryllium foil obtained in the procedure B4 as a new workpiece. In addition, since the sheath becomes harder as the number of passes increases, the number of passes is set within a range in which the ductility of the sheath is empirically maintained. Note that the procedures B2 to B5 are the same as the procedures A3 to A6 described above.
［実施例１］
第１の圧延工程から第２の圧延工程へ切り替えるしきい値を６０μｍとし、目標厚み１０μｍ及び１５μｍのベリリウム箔を製作した。圧延温度は６５０−７００℃とし、シースにはステンレス鋼ＳＵＳ３０４材を使用した。１〜６ｃｈまでは第１の圧延工程を採用したが、６ｃｈ終了後にベリリウム箔の厚さがしきい値である６０μｍ以下になったため、７ｃｈ以降は第２の圧延工程を採用し、目標厚みとなるまで圧延を行った。作業完了後の作業完了後のベリリウム箔の欠陥密度を求めたところ、１０μｍで０．６８個／ｃｍ2、１５μｍで０．０５個／ｃｍ2であった（表１参照）。欠陥は丸穴であり、破断箇所（裂け目）は見られなかった。なお、欠陥密度は、現像フィルムを見るための白色光源の上にベリリウム箔を置き、光が透過した箇所（欠陥）の総数を計測し、ベリリウム箔の面積でその総数を除した値とした。また、作業完了後のベリリウム箔のホウ素残留の有無を確認するために、ＳＥＭを使用し、５００倍で観察したところ、ＢＮの残留が認められず、更に、ＥＤＸを使用し、表面の定性分析を行なったが、Ｂ及びＮの検出ピークは認めらなかった。この作業完了後のベリリウム箔から欠陥個数のゼロの領域を切り出し（面積１０００ｍｍ2）、アルバック社製のヘリウムリークディテクターを用いて、空気の漏れ量を測定した。測定した結果、リークレートは１×１０-10Ｐａ・ｍ3／ｓｅｃ以下であった。
[Example 1]
The threshold value for switching from the first rolling process to the second rolling process was set to 60 μm, and beryllium foils having target thicknesses of 10 μm and 15 μm were manufactured. The rolling temperature was 650-700 ° C., and stainless steel SUS304 material was used for the sheath. The first rolling process was adopted for 1 to 6 ch, but the thickness of the beryllium foil became the threshold value of 60 μm or less after the completion of 6 ch, so the second rolling process was adopted after 7 ch until the target thickness was reached. Rolled. When the defect density of the beryllium foil after completion of the work was determined, it was 0.68 pieces / cm 2 at 10 μm and 0.05 pieces / cm 2 at 15 μm (see Table 1). The defect was a round hole, and no fractured portion (fissure) was found. The defect density was a value obtained by placing the beryllium foil on a white light source for viewing the developed film, measuring the total number of locations (defects) through which light was transmitted, and dividing the total by the area of the beryllium foil. In addition, in order to confirm the presence or absence of boron residue in the beryllium foil after completion of the work, when observing at 500 times using SEM, no BN residue was observed, and further, EDX was used to qualitatively analyze the surface. However, no detection peaks for B and N were observed. A region having zero defects was cut out from the beryllium foil after completion of this operation (area: 1000 mm 2 ), and the amount of air leakage was measured using a helium leak detector manufactured by ULVAC. As a result of the measurement, the leak rate was 1 × 10 −10 Pa · m 3 / sec or less.
［実施例２］
第１の圧延工程から第２の圧延工程へ切り替えるしきい値を２５μｍとし、目標厚み１０μｍ及び１５μｍのベリリウム箔を製作した。圧延温度は６５０−７００℃とし、シースにはステンレス鋼ＳＵＳ３０４材を使用した。１〜９ｃｈまでは第１の圧延工程を採用したが、９ｃｈ終了後にベリリウム箔の厚さがしきい値である２５μｍ以下になったため、１０ｃｈ以降は第２の圧延工程を採用し、目標厚みとなるまで圧延を行った。作業完了後のベリリウム箔の欠陥密度を求めたところ、１０μｍで０．４１個／ｃｍ2、１５μｍで０．０３個／ｃｍ2であった（表１参照）。欠陥は丸穴であり、破断箇所（裂け目）は見られなかった。なお、欠陥密度は、実施例１と同じ方法で計測した。また、作業完了後のベリリウム箔のホウ素残留の有無を確認するために、ＳＥＭを使用し、５００倍で観察したところ、ＢＮの残留が認められず、更に、ＥＤＸを使用し、表面の定性分析を行なったが、Ｂ及びＮの検出ピークは認めらなかった。この作業完了後のベリリウム箔から欠陥個数のゼロの領域を切り出し（面積１５００ｍｍ2）、アルバック社製のヘリウムリークディテクターを用いて、空気の漏れ量を測定した。測定した結果、リークレートは１×１０-10Ｐａ・ｍ3／ｓｅｃ以下であった。
[Example 2]
A threshold value for switching from the first rolling process to the second rolling process was set to 25 μm, and beryllium foils having target thicknesses of 10 μm and 15 μm were manufactured. The rolling temperature was 650-700 ° C., and stainless steel SUS304 material was used for the sheath. The first rolling process was adopted up to 1 to 9 ch, but after the completion of 9 ch, the thickness of the beryllium foil became 25 μm or less, which is the threshold value, and the second rolling process was adopted after 10 ch until the target thickness was reached. Rolled. The defect density of the beryllium foil after completion of the work was determined to be 0.41 / cm 2 at 10 μm and 0.03 / cm 2 at 15 μm (see Table 1). The defect was a round hole, and no fractured portion (fissure) was found. The defect density was measured by the same method as in Example 1. In addition, in order to confirm the presence or absence of boron residue in the beryllium foil after completion of the work, when observing at 500 times using SEM, no BN residue was observed, and further, EDX was used to qualitatively analyze the surface. However, no detection peaks for B and N were observed. A region having zero defects was cut out from the beryllium foil after completion of this operation (area 1500 mm 2 ), and the amount of air leakage was measured using a helium leak detector manufactured by ULVAC. As a result of the measurement, the leak rate was 1 × 10 −10 Pa · m 3 / sec or less.
［実施例３］
第１の圧延工程から第２の圧延工程へ切り替えるしきい値を１５μｍとし、目標厚み１０μｍのベリリウム箔を製作した。圧延温度は６５０−７００℃とし、シースにはステンレス鋼ＳＵＳ３０４材を使用した。１〜１１ｃｈまでは第１の圧延工程を採用したが、１１ｃｈ終了後にベリリウム箔の厚さがしきい値である１５μｍ以下になったため、１２ｃｈ以降は第２の圧延工程を採用し、目標厚みとなるまで圧延を行った。作業完了後のベリリウム箔の欠陥密度を求めたところ、０．３１個／ｃｍ2であった（表１参照）。欠陥は丸穴であり、破断箇所（裂け目）は見られなかった。なお、欠陥密度は、実施例１と同じ方法で計測した。また、作業完了後のベリリウム箔のホウ素残留の有無を確認するために、ＳＥＭを使用し、５００倍で観察したところ、ＢＮの残留が認められず、更に、ＥＤＸを使用し、表面の定性分析を行なったが、Ｂ及びＮの検出ピークは認めらなかった。この作業完了後のベリリウム箔から欠陥個数のゼロの領域を切り出し（面積１８００ｍｍ2）、アルバック社製のヘリウムリークディテクターを用いて、空気の漏れ量を測定した。測定した結果、リークレートは１×１０-10Ｐａ・ｍ3／ｓｅｃ以下であった。
[Example 3]
A threshold value for switching from the first rolling process to the second rolling process was set to 15 μm, and a beryllium foil having a target thickness of 10 μm was manufactured. The rolling temperature was 650-700 ° C., and stainless steel SUS304 material was used for the sheath. The first rolling process was adopted up to 1 to 11 ch, but after the end of 11 ch, the thickness of the beryllium foil became the threshold value of 15 μm or less, so the second rolling process was adopted after 12 ch until the target thickness was reached. Rolled. The defect density of the beryllium foil after the completion of the work was found to be 0.31 piece / cm 2 (see Table 1). The defect was a round hole, and no fractured portion (fissure) was found. The defect density was measured by the same method as in Example 1. In addition, in order to confirm the presence or absence of boron residue in the beryllium foil after completion of the work, when observing at 500 times using SEM, no BN residue was observed, and further, EDX was used to qualitatively analyze the surface. However, no detection peaks for B and N were observed. A region with zero defects was cut out from the beryllium foil after completion of this operation (area: 1800 mm 2 ), and the amount of air leakage was measured using a helium leak detector manufactured by ULVAC. As a result of the measurement, the leak rate was 1 × 10 −10 Pa · m 3 / sec or less.
［比較例１］
１ｃｈ目からすべて第２の圧延工程（つまりＢＮ不使用）を実施し、ベリリウム箔の厚さが１０μｍとなったところで作業を完了したところ、作業完了後のベリリウム箔の欠陥密度は７．０２個／ｃｍ2であった（表１参照）。これは、実施例１〜３の欠陥密度の約１０〜２０倍である。また、作業完了後のベリリウム箔から欠陥個数のゼロの領域をできるだけ大面積となるように選び出したところ、その面積は１００ｍｍ2程度であった。こうして得られた欠陥個数ゼロのベリリウム箔につき、空気の漏れ量を測定したところ、７×１０-9Ｐａ・ｍ3／ｓｅｃであった。
[Comparative Example 1]
The second rolling process (that is, no BN) was performed from the first channel, and the work was completed when the thickness of the beryllium foil reached 10 μm. The defect density of the beryllium foil after the work was 7.02 / Cm 2 (see Table 1). This is about 10 to 20 times the defect density of Examples 1 to 3. Further, when the area having zero defects was selected from the beryllium foil after completion of the operation so as to have as large an area as possible, the area was about 100 mm 2 . With respect to the beryllium foil having zero defects thus obtained, the amount of air leakage was measured and found to be 7 × 10 −9 Pa · m 3 / sec.
ここで、実施例１〜３につき、しきい値（第１の圧延工程と第２の圧延工程を切り替える厚み）と厚み１０μｍでの欠陥密度との関係を示すグラフを図２に示す。第１の圧延工程が目標厚みに近いところまで実施されるほど欠陥密度が小さくなることが分かる。実施例１〜３の欠陥は丸穴であったため、圧延工程でシースがベリリウム箔に押し込まれたことにより発生したと考えられる。また、実施例１〜３では、シースの材料としてＳＵＳ３０４（カーボン含有量 規格値０．０８重量％以下、実測値０．０７重量％）を採用したが、ＳＵＳ３０４Ｌ（カーボン含有量 規格値０．０３重量％以下、実測値０．０２重量％）を採用すれば、シースからの粒子の脱落を有効に防止することができるため、欠陥密度が一層小さくなると推察される。ここで、ＳＵＳ３０４の小片とＳＵＳ３０４Ｌの小片を、電気炉にて７００℃で６０分熱処理を施した後、ＪＩＳ Ｇ０５７１（ステンレス鋼のシュウ酸エッチング試験）に準じた耐腐食性試験を実施した。具体的には、熱処理を施した試験片を樹脂に埋め込んだ後、鏡面研磨を施し、シュウ酸で腐食させ、光学顕微鏡（４００倍）でミクロ観察して腐食程度を評価した。そうしたところ、ＳＵＳ３０４Ｌの小片では、腐食後も熱処理前の結晶構造を維持していたのに対し、ＳＵＳ３０４の小片では、粒界が際立ってくっきりと見え、鋭敏化により脆弱となり、粒子が脱落しやすい状態になった。このことから、ＳＵＳ３０４Ｌ製のシースを使用すれば、実施例１〜３に比べて欠陥密度が一層小さくなるといえる。 Here, for Examples 1 to 3, a graph showing the relationship between the threshold value (thickness at which the first rolling process and the second rolling process are switched) and the defect density at a thickness of 10 μm is shown in FIG. 2. It can be seen that the defect density decreases as the first rolling process is performed to a point near the target thickness. Since the defect of Examples 1-3 was a round hole, it is thought that it generate | occur | produced when the sheath was pushed into beryllium foil at the rolling process. In Examples 1 to 3, SUS304 (carbon content standard value 0.08% by weight or less, measured value 0.07% by weight) was adopted as the material of the sheath, but SUS304L (carbon content standard value 0.03%). If the weight% or less and the measured value 0.02% by weight) are employed, it is presumed that the particle density from the sheath can be effectively prevented, so that the defect density is further reduced. Here, the SUS304 piece and the SUS304L piece were heat-treated at 700 ° C. for 60 minutes in an electric furnace, and then subjected to a corrosion resistance test according to JIS G0571 (stainless steel oxalic acid etching test). Specifically, after the heat-treated test piece was embedded in the resin, it was mirror-polished, corroded with oxalic acid, and microscopically observed with an optical microscope (400 times) to evaluate the degree of corrosion. As a result, the SUS304L small piece maintained the crystal structure before the heat treatment even after corrosion, whereas the SUS304 small piece made the grain boundary stand out clearly, became fragile due to sensitization, and the particles easily fall off. It became a state. From this, it can be said that if a sheath made of SUS304L is used, the defect density is further reduced as compared with Examples 1-3.
本発明は、非常に薄いベリリウム箔が要求される技術分野、例えばＸ線用窓材や電子線用窓材に利用可能である。 The present invention can be used in technical fields where very thin beryllium foil is required, for example, X-ray window materials and electron beam window materials.
Claims (5)
ベリリウム箔とステンレス鋼からなる一対のシースとの間に固体潤滑剤である窒化ホウ素（ＢＮ）を塗布してなる積層体を作製し、該積層体の熱間圧延加工を繰り返し行う、第１の圧延工程と、ベリリウム箔とステンレス鋼からなる一対のシースとの間にＢＮを塗布することなく積層体を作製し、該積層体の熱間圧延加工を繰り返し行う、第２の圧延工程と、を実行するにあたり、
ベリリウム箔の厚さが１５〜６０μｍの間で定められた所定のしきい値（厚み）以下になっていない場合には、前記第１の圧延工程を繰り返し実行し、その後、ベリリウム箔の厚さが前記しきい値以下になった場合には、前記第２の圧延工程をベリリウム箔の厚さが５〜２０μｍの間で前記しきい値より小さい値に定められた目標厚さになるまで繰り返し実行する、
超薄膜ベリリウム箔の製造方法。 A method for producing the ultra-thin beryllium foil according to any one of claims 1 to 3,
A laminated body formed by applying boron nitride (BN), which is a solid lubricant, between a beryllium foil and a pair of sheaths made of stainless steel is manufactured, and hot rolling of the laminated body is repeatedly performed. A second rolling step in which a laminate is produced without applying BN between a rolling step and a pair of sheaths made of beryllium foil and stainless steel, and hot rolling of the laminate is repeated. In doing so,
When the thickness of the beryllium foil is not less than or equal to a predetermined threshold value (thickness) set between 15 and 60 μm, the first rolling step is repeatedly performed, and then the thickness of the beryllium foil Is less than the threshold value, the second rolling process is repeated until the thickness of the beryllium foil is between 5 and 20 μm and reaches a target thickness that is set to a value smaller than the threshold value. Run,
Manufacturing method of ultra-thin beryllium foil.
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| RU2739457C1 (en) * | 2019-06-26 | 2020-12-24 | Акционерное общество "Высокотехнологический научно-исследовательский институт неорганических материалов имени академика А.А. Бочвара" | Method of producing thin vacuum-tight beryllium foil |
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| CN113877980A (en) * | 2021-10-22 | 2022-01-04 | 西北稀有金属材料研究院宁夏有限公司 | Beryllium window material and preparation method thereof |
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| RU2739457C1 (en) * | 2019-06-26 | 2020-12-24 | Акционерное общество "Высокотехнологический научно-исследовательский институт неорганических материалов имени академика А.А. Бочвара" | Method of producing thin vacuum-tight beryllium foil |
| WO2020263127A1 (en) * | 2019-06-26 | 2020-12-30 | Акционерное общество "Высокотехнологический научно-исследовательский институт неорганических материалов имени академика А.А. Бочвара" | Method for producing vacuum-tight beryllium foil |
| WO2020263128A1 (en) * | 2019-06-26 | 2020-12-30 | Акционерное общество "Высокотехнологический научно-исследовательский институт неорганических материалов имени академика А.А. Бочвара" | Method for producing thin vacuum-tight beryllium foil |
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